Rapid Borate Fusion Pre-treatment for ICP-AES Determination of Tungsten in High-speed Steel

2020

ISIJ Int.

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This paper suggests an improved method for the sample preparation to quantify vanadium in high-speed steel by using flame atomic absorption spectrometry. The suggested method prepared a solidified glass body fused with lithium tetraborate after the sample was decomposed with an acid mixture of hydrofluoric and nitric acids. The obtained borate glass was easily dissolved with nitric acid without any residues. Another novelty of this paper was a simultaneous measurement of a vanadium absorption line and a nickel absorption line in the close wavelength, when a multiwavelength high-resolution spectrometer system was employed. The nickel line worked as an internal standard and could contribute to more precise quantification of vanadium in high-speed steel samples.

Section: Introductionmentioning

confidence: 99%

Borate Fusion Preparation of High-speed Steel for Determination of Vanadium by Flame Atomic Absorption Spectrometry with a Continuum-light-source Spectrometer System

2020

ISIJ Int.

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“…It is difficult to digest a tool steel sample without remaining a residue and precipitating no tungsten hydrate. 1) For example, an acid mixture containing hydrochloric and nitric acids, 2) which easily digests a stainless steel sample, cannot completely decompose metal carbides and oxides (e.g., aluminum, calcium, and chromium 3) ) in a steel sample. Digestion of such carbides and oxides should be conducted by fusion procedures with potassium disulfate 4) and sodium carbonate.…”

Section: Introductionmentioning

confidence: 99%

“…Digestion of such carbides and oxides should be conducted by fusion procedures with potassium disulfate 4) and sodium carbonate. 5) Authors were previously suggested lithium tetraborate fusion procedures for a high-speed tool steel sample on ICP-AES 1) and X-ray fluorescence 6,7) analyses. Although these methods were successfully employed to determine alloyed elements, they cannot be applied for sulfur quantification because of the loss of sulfur during its fusion process.…”

Section: Introductionmentioning

confidence: 99%

Application of Quaternary Acid Mixture to Microwave Digestion Effective for Various Kinds of Steel Samples

2020

ISIJ Int.

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This paper suggests a procedure of an improved digestion method, which can be applied to a variety of steel samples, for preparing the sample solution to quantify alloyed elements and sulfur simultaneously in inductively coupled plasma atomic emission spectrometry. A conventional digestion method using a mixture of hydrochloric and nitric acid has a poor ability to decompose tool steel completely. Alternatively, a microwave digestion method, in which an acid mixture of hydrochloric acid, hydrofluoric acid, nitric acid, and phosphoric acid was prepared with 1:1:1:1 volume ratio, enabled various steel samples including tool steel and stainless steel to be fully decomposed. Due to no addition of sulfuric acid, the sulfur content in the samples could be determined. The suggested procedure was applicable to determine sulfur, vanadium, chromium, manganese, cobalt, nickel, molybdenum, and tungsten in a variety of steel alloys using the same dissolution procedure.

“…The quantitative analysis of high‐speed steel, which is a kind of high‐alloyed steel designed for cutting tools or heat jigs, is normally employed by inductively coupled plasma‐atomic emission spectrometry (ICP‐AES) . This ICP‐AES procedure, which always needs a pretreatment of samples using acid decomposition, is tedious and time‐consuming.…”

Section: Introductionmentioning

confidence: 99%

Absorption‐free calibration on X‐ray fluorescence analysis of high‐speed steel with glass bead preparation

2019

X-Ray Spectrometry

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This article describes a novel idea on preparation of a glass bead for X-ray fluorescence spectrometry, to determine alloyed elements in high-speed steel without any matrix correction. The quantification method using the glass bead is generally effective to reduce secondary X-ray absorption and enhancement (matrix effect) by coexisting elements in a sample. Although the glass bead is normally prepared based on a flux-to-sample ratio, the suggested method mainly controls an absolute amount of the sample in the glass bead to prevent from any interference with the matrix elements. As a result, the alloyed elements, except tungsten, in high-speed steels could be determined with high precision and accuracy, independent of the flux-to-sample ratio. However, the fluorescent X-ray intensity of tungsten Lα line (8.40 keV) was obviously influenced by the sample amount (iron content) in a glass bead; in this case, the Mα line (1.77 keV) could be employed alternatively.